CN102897750B - PrPrearation method for graphene film - Google Patents
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- CN102897750B CN102897750B CN201110215856.7A CN201110215856A CN102897750B CN 102897750 B CN102897750 B CN 102897750B CN 201110215856 A CN201110215856 A CN 201110215856A CN 102897750 B CN102897750 B CN 102897750B
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Abstract
The invention discloses a preparation method for a graphene film. The method comprises the steps of putting small sheets of the in advance synthetic graphene film on a substrate, and growing the graphene film on the substrate by using the small sheets of the in advance synthetic graphene film as induced points for the growth of s large-area graphene film and adopting carbon atoms released by carbon atom-containing gas carbon source, solid carbon source, liquid carbon source or composite carbon source materials thereof. The graphene film can directly grow on the substrate of practical application graphene film, so that the graphene film needs not to be transferred when being used. The number of layers, the structure and the size of the prepared graphene film are easy to control; the temperature for growing the graphene film can be 0 DEG C-2000 DEG C; the prepared graphene film has excellent photoelectric characteristics and is suitable for large-scale manufacture of optoelectronic devices.
Description
Technical field
The present invention relates to graphene film, relate in particular to a kind of preparation method of graphene film.
Background technology
Graphene is that mono-layer graphite is otherwise known as by the former molecular two-dirnentional structure material of cellular monolayer carbon; In physical property, it has been generally acknowledged that the material that ten layers of above Graphene are piled up is exactly the graphite of three-dimensional structure, carbon nanotube is by Graphene, to be rolled into the monodimension nanometer material of tubbiness.Graphene has remarkable two-dimentional electricity, optics, calorifics, mechanical property and chemical stability, the two-dirnentional structure that it is unique and excellent crystallography quality make it at supper-fast micro-nano opto-electronic device, radio-frequency devices, the fields such as clear energy sources and various kinds of sensors have important practical value.Such as, electronics is followed relativistic quantum mechanics in Graphene, there is no rest mass, ultraspeed operation with 1/300 light velocity, show unusual room temperature quantum hall effect and ballistic transport phenomenon, can prepare room temperature ballistic transport transistor, be regarded as the important foundation novel material of Future Information nano-device; Graphene electric transmission speed is 150 times of silicon, is expected to supper-fast computer and radio-frequency devices that the speed of preparing reaches megahertz; The susceptibility of the unit molecule degree of Graphene is expected at various sensors, as being used widely in the fields such as gas sensor and biosensor; Graphene has the optical characteristics of 2.3% photoabsorption, make it can be for the preparation of supper-fast photo-detector and mode locked laser, on the other hand, due to extremely low optical absorption characteristics, make Graphene both can be used for preparing opto-electronic device, as the transparency electrode of photodiode and solar cell etc., thereby replace cost costliness, resource scarcity, not foldingly take the ITO nesa coating that indium is main component, also can be used for preparing ultracapacitor and lithium ion battery; The effciency of energy transfer of the solar battery based on Graphene is expected to reach 24%.
The preparation method of graphene film comprise mechanically peel method [K. S. Novoselov,
et al. Science 306,666 (2004) .], solution stripping method [X. L. Li, et al. Science 319,1229 (2008) .], chemistry redox method [D. A. Dikin, et al. Nature 448,457 (2007). Z. S. Wu, et al. Carbon 47,493 (2009) .], silicon carbide thermal decomposition method [C. Berger
et al. Science 312,1191 (2006); A. Tzalenchuk, et al. Nature Nanotechnol 5,186 (2010) .], chemical Vapor deposition process (CVD) [C. A. Di, et al. Adv. Mater. 20,3289 (2008); A. Reina, et al. Nano Lett. 9,30 (2009); K. S. Kim, et al. Nature 457,706 (2009) .], carbon segregation method (segregation) etc.The shape of the graphene film that wherein mechanically peel method, solution stripping method and chemistry redox method are prepared is all random substantially, and the number of plies of graphene film and size are difficult to control; Although mechanically peel method can produce the Graphene of perfect lattice, be only adapted to fundamental research, be not suitable for large-scale application.Silicon carbide thermal decomposition method is a kind of method of solid carbon source growing graphene film, its basic step is included under ultrahigh vacuum(HHV), pyroprocessing silicon carbide with 1400 ℃ of left and right, Siliciumatom is evaporated and allow carbon atom form graphene film at silicon carbide, this method requires very high, very harsh to preparation condition, and is difficult to obtain the single uniform graphene film of the number of plies.Chemical Vapor deposition process (CVD) is to use gaseous carbon source growing graphene film on metal catalytic layer, except utilizing gaseous carbon source, also utilize solid carbon source [J. M. Tour,
et al.nature 468,549 (2010)] and liquid carbon source [F. Muller,
et al.small 5,2291 (2009); Y. Miyata,
et al.applied Physics Letters 96,263105 (2010)] adopt and to be similar to chemical Vapor deposition process and to have synthesizing graphite alkene film on the substrate of metal catalytic.Carbon segregation method (segregation) is first carbon atom to be doped in metal catalytic layer, then through Overheating Treatment, carbon atom is disengaged from metal catalytic layer, thereby forms graphene film in metallic surface.
Chemical Vapor deposition process and carbon segregation method can big area synthesizing graphite alkene films, and can control preferably to a certain extent the number of plies of graphene film, be adapted to large-scale application, but must adopt metal catalytic layer and on this metal catalytic substrate synthesizing graphite alkene film, synthesis temperature is generally more than 650 ℃.Like this, big area graphene film synthetic in metal substrate must be transferred to other target substrate as just used graphene film in insulating substrate during practical application graphene film; Big area shifts graphene film and also has very large challenge at present, therefore, if the substrate that has technological method graphene film can be grown directly upon to be applicable to graphene film particular application technology is as in isolator or semiconducter substrate, to not need transfer step, also can avoid the variation of the graphene film texture quality that caused by transfer process; This will speed up Graphene technical development and practical application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of simple preparation method who is suitable for the graphene film of large area deposition is provided, for this reason, the present invention is by the following technical solutions: from pre-synthesis graphene film, choose a small pieces graphene film, described small pieces graphene film is transferred to conductor, the starting point of growing as induction graphene film on the substrate of semi-conductor or isolator, on described substrate, adopt and come from solid carbon source, liquid carbon source, the carbon atom that in gaseous carbon sources or aforementioned carbon source, two or more mixed carbon source discharges arbitrarily be take small pieces graphene film as starting point growing graphene film.
The graphene film small pieces of described conduct induction graphene film large area deposition be selected from by micromechanics peel off, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.
Described conduct is inorganic materials, organic polymer material or its matrix material that is suitable for graphene film particular application technology for conductor, semi-conductor or the insulator substrates of large area deposition graphene film, such as: be metal or alloy; For preparing at present Si, Ge, Ge-Si, Se, GaN, GaAs, GaAsN, InP, ZnS, CdTe, HgTe, InAs-InP, GaAs-GaP, the ZnGeP of semiconducter device
2, ZnGeAs
2, CdGeAs
2, CdSnSe
2, CuGaSe
2, AgInTe
2, AgTlTe
2, CuInSe
2, CuAlS
2, Cu
3asSe
4, Ag
3asTe
4, Cu
3sbS
4, Ag
3sbSe
4, Cu
2feSnS
4, the inorganic semiconductor material such as ZnO, CuO and pentacene, poly--3 alkylthrophenes of P3HT(), C
60, PCBM, PPV(be poly-to vinylbenzene), the organic semiconductor material such as naphthalene, anthracene, polyacrylonitrile, phthalocyanine; For SiO
2, Al
2o
3, HfO
2, BN, SiN
x, the insulating material such as SiC, AlN, mica, glass, pottery, sapphire, polyvinyl alcohol, poly-(4-Vinyl phenol), divinyl tetramethyl disiloxane-bis-(benzocyclobutene), polyethylene terephthalate (PET), polymethylmethacrylate (PMMA), Derlin, chloroprene rubber, polyvinyl chloride, styrene-butadiene rubber(SBR), polymeric amide, trimeric cyanamide, polyethylene, tetrafluoroethylene, but be not limited to above material.
Described gaseous carbon source, solid-state carbon source, liquid carbon source material or mixed carbon source material refer to containing easily discharging the material of the carbon atoms of carbon atom, comprise that alkane is as methane etc., alkene is as ethene etc., alkynes is as acetylene etc., and aromatic hydrocarbon is as benzene, and alcohol is as ethanol etc., ketone is as acetone etc., graphite, the material of the carbon containings such as carbon pipe, but be not limited to above material.
The method that the described carbon source material from carbon atoms discharges carbon atom is through Overheating Treatment, sputtering method, laser treatment, Cement Composite Treated by Plasma or decomposition reaction.
The shape of the graphene film small pieces of described conduct induction point can be arbitrary shape, such as square, rectangle, circle, ellipse or irregular type; As inducing the number of plies of the graphene film small pieces of point, be 1 layer to 200 layers, be preferably 1 layer to 20 layers, optimum is 1 layer to 5 layers; As inducing the area of the graphene film small pieces of point, be 1nm
2to 50000cm
2, optimum is 1nm
2to 1000cm
2, the most optimum is 1nm
2to 100um
2.
The number of plies of the described graphene film of growing in conductor, semi-conductor or insulator substrates is 1 layer to 200 layers, is preferably 1 layer to 20 layers, and optimum is 1 layer to 5 layers.
The temperature of growing graphene film is 0 ℃ to 2000 ℃, is preferably 50 ℃ to 1000 ℃, and optimum is 50 ℃ to 600 ℃.
The method of preparing graphene film of the present invention is to adopt pre-synthesis graphene film sheet and induce graphene film large area deposition; Because graphene film small pieces can be placed on conductor, semi-conductor or insulator substrates, thus can be in any target substrate large area deposition graphene film, just do not need to shift again like this graphene film during using mineral carbon alkene film; The underlayer temperature of growing graphene film can be suitable for low-temperature epitaxy graphene film between 50 ℃ to 600 ℃, is compatible with existing semi-conductor industry; The thickness of graphene film, structure, size are easily controlled; Prepare graphene film and there is excellent photoelectric characteristic, be applicable to manufacture on a large scale high performance opto-electronic device.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the present invention prepares graphene film: (a) from pre-synthesis graphene film, extract small pieces and transfer on substrate, (b) take the small pieces graphene film that shifts is induction point, utilizes carbon atom by the gaseous carbon source that contains carbon atom, liquid carbon source, solid-state carbon source or its mixed carbon source material production at Grown graphene film;
Fig. 2 is for usining single-layer graphene prepared by mechanically peel method as the small pieces Graphene that brings out Graphene large area deposition, at SiO
2the optical microscope image of Grown single-layer graphene;
Fig. 3 is for usining double-layer graphite alkene prepared by chemical gaseous phase depositing process as the small pieces Graphene that brings out Graphene growth, at the Raman collection of illustrative plates of polymer P ET Grown double-layer graphite alkene;
Fig. 4 is for take single-layer graphene prepared by mechanically peel method as bringing out the small pieces Graphene of Graphene growth, at the scanning electron microscope image of Au Grown single-layer graphene;
Fig. 5 is for usining minority layer graphene film prepared by redox chemical process as the small pieces graphene film that brings out Graphene growth, at the Auger electron collection of illustrative plates of Si Grown graphene film.
Embodiment
As shown in Figure 1, the preparation method of graphene film adopts from pre-synthesis graphene film 1, to select a small pieces graphene film 2, the small pieces graphene film of choosing is positioned on the substrate 3 that is adapted to graphene film particular application technology, utilize come from the carbon atom 4 that discharges in gaseous carbon source, liquid carbon source, solid-state carbon source or its mixed carbon source material that contains carbon atom and on substrate 3 growing graphene film 5.
Described graphene film sheet be select in being peeled off by micromechanics, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.As bring out graphene film growth graphene film sheet be shaped as square, rectangle, circle, ellipse or irregular type; As the number of plies of bringing out the graphene film sheet of graphene film growth, be 1 layer to 200 layers, optimum is 1 layer to 20 layers, and the most optimum is 1 layer to 5 layers; As the area that brings out the graphene film sheet of graphene film growth, be 1nm
2to 50000 cm
2, optimum is 1nm
2to 1000 cm
2, the most optimum is 1nm
2to 100um
2.Described substrate material is inorganic or organic conductor, semi-conductor, isolator or its matrix material that is applicable to graphene film particular application technology.Described gaseous carbon source, solid-state carbon source, liquid carbon source material or its mixed carbon source refer to containing the material by carbon atom, optimum for easily discharging the material of carbon atom.The number of plies of the described graphene film at Grown is 1 layer to 200 layers, and optimum is 1 layer to 20 layers, and the most optimum is 1 layer to 5 layers.
Embodiment 1: utilize single-layer graphene prepared by mechanically peel method as the Graphene small pieces of induction Graphene large area deposition, at SiO
2grown graphene film
Utilize the Scotch adhesive tape of 3M company adopt mechanically peel method from Pintsch process graphite-made for single-layer graphene, and transfer to SiO
2on substrate, the graphene film small pieces of Graphene growth are brought out in conduct; The SiO of graphene film small pieces will be had
2substrate is positioned in ultrahigh vacuum(HHV) (6.0 * 10
-9torr) carry out 1000 oC thermal treatment 5 minutes; Subsequently, at the logical H of 800oC
2with C
2h
4mixed gas, at SiO
2graphene small pieces induction Graphene growth on substrate 5 minutes; Finally drop to room temperature, thereby at SiO
2substrate large area deposition single-layer graphene (Fig. 2).
Effect: SiO
2the important dielectric materials of contemporary silica-based electron device, numeral/logical circuit, directly at SiO
2insulating substrate growing graphene film, will speed up the integrated of Graphene technology and contemporary optoelectronics industry, reduces costs.
Embodiment 2: utilize the double-layer graphite alkene of being prepared by chemical gaseous phase depositing process as the Graphene small pieces of inducing Graphene large area deposition, on polymer poly ethylene glycol terephthalate (PET) substrate, prepare graphene film
The Cu sheet that after polishing and surface treatment, 25um is thick is positioned in high vacuum to (1.0 * 10
-8torr) carry out 1000 oC thermal treatment 30 minutes; Subsequently, logical CH
4gas and H
2gas growth 2 minutes; With the rate of temperature fall of 15oC/ minute by the near room temperature of temperature, thereby on Cu film, obtain double-layer graphite alkene.From Cu, shift a fritter Graphene upper to polymer P ET: spin coating 500nm polymethylmethacrylate (PMMA) layer on synthetic Graphene surface, Graphene/the Cu that scribbles PMMA is positioned in iron nitrate solution Cu erosion to fall, thereby obtain PMMA/ Graphene, then PMMA/ Graphene is transferred on PET, with acetone solution, fall PMMA subsequently, small pieces double-layer graphite alkene has been transferred on PET like this.
Using Ar gas as carrier, by producing carbon atom by liquid ethanol, be incorporated into the PET substrate zone that is placed with a fritter graphene film that temperature is 100oC, thereby with this Graphene small pieces induction graphene film large area deposition (Fig. 3) on PET.
Effect: various flat pannel display, touch screen and solar cell etc. all need ELD, flexible device is more and more attracted attention, PET is transparent flexible materials, directly under lower temperature, the Graphene of transparent conduction is grown on PET, for development soft graphite alkene conductive, transparent membrane technique is laid a good foundation.
Embodiment 3: single-layer graphene prepared by the mechanically peel method of usining is as the Graphene small pieces of induction Graphene large area deposition, at golden substrate growing graphene
Utilize the Scotch adhesive tape of 3M company adopt mechanically peel method from Pintsch process graphite-made for single-layer graphene, and transfer on Au substrate as the Graphene small pieces of inducing Graphene large area deposition on Au.The Au substrate that is loaded with Graphene small pieces is positioned over to sputtering chamber, adopt sputtering method that carbon atom is splashed on Au substrate from agraphitic carbon target, thereby the Graphene small pieces that shift have brought out on Au substrate growing graphene (Fig. 4) under the underlayer temperature of 300 oC.
Effect: gold waits the resource-constrained of noble metal material, and Graphene has excellent physical strength and the transparency, on the surface of gold etc., directly plating one layer graphene contributes to protect golden precious materials.
Embodiment 4: minority layer graphene film prepared by the redox chemical process of usining is as the Graphene small pieces of induction Graphene large area deposition, at Si Grown graphene film
Adopt redox chemical process that graphite oxidation is become to graphite oxide, graphite oxide is through supersound process and centrifugal and graphite oxide is split up into graphene oxide; Then graphene oxide being inserted to pure hydrazine solution obtains through reduction reaction as the Graphene small pieces of induction Graphene large area deposition; Small pieces graphene film is transferred on Si substrate and brought out graphene film growth.
To there is the Si substrate of graphene film small pieces to be placed in sputtering chamber, adopt laser pulse method that carbon atom is splashed on Si substrate from agraphitic carbon target, thereby take graphene film small pieces as starting point is at Si Grown graphene film (Fig. 5).
Effect: Si is the core material of contemporary silica-based electron device, numeral/logical circuit, directly at semiconducter substrate growing graphene films such as Si, will speed up the integrated of Graphene technology and contemporary optoelectronics industry, reduces costs.
Above-described embodiment is only not used in and limits the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (17)
1. the preparation method of a graphene film, it is characterized in that choosing a small pieces graphene film (2) from pre-synthesis graphene film (1), described small pieces graphene film (2) is transferred to conductor, the upper starting point as the growth of induction graphene film of the substrate of semi-conductor or isolator (3), upper employing of described substrate (3), come from solid carbon source, liquid carbon source, the carbon atom (4) that in gaseous carbon sources or aforementioned carbon source, two or more mixed carbon source discharges arbitrarily be take small pieces graphene film (2) as starting point growing graphene film (5),
The method that discharges carbon atom from the carbon source material of carbon atoms be to react through Overheating Treatment, sputtering method, laser treatment, Cement Composite Treated by Plasma or decomposition.
2. the preparation method of graphene film according to claim 1, it is characterized in that described pre-synthesis graphene film (1) be by micromechanics peel off, liquid phase is peeled off, chemical vapour deposition, carbon segregation, chemistry redox reaction, decompose solid-phase carbon source or decompose the method for phase carbon source and synthetic graphene film.
3. the preparation method of graphene film according to claim 1, what it is characterized in that described small pieces graphene film (2) is shaped as square, rectangle, circle, ellipse or irregular type.
4. the preparation method of graphene film according to claim 1, is characterized in that the number of plies of described small pieces graphene film (2) is 1 layer to 200 layers.
5. the preparation method of graphene film according to claim 1, is characterized in that described small pieces graphene film (2) area is 1nm
2to 50000cm
2.
6. the preparation method of graphene film according to claim 1, is characterized in that take that small pieces graphene film (2) is as inducing the required carbon atom (4) of some large area deposition graphene film (5) to come from any two or more mixed carbon source material in the gaseous carbon source that contains carbon atom of easy generation carbon atom, solid-state carbon source, liquid carbon source material or aforementioned carbon source.
7. the preparation method of graphene film according to claim 1, is characterized in that the carbon atom of described release is at the Grown graphene film that has pre-synthesis small pieces graphene film.
8. the preparation method of graphene film according to claim 1, is characterized in that the number of plies of the graphene film (5) that becomes at Grown is 1 layer to 200 layers.
9. the preparation method of graphene film according to claim 1, the temperature that it is characterized in that growing graphene film (5) is 0 ° of C to 2000 ° of C.
10. the preparation method of graphene film according to claim 1, is characterized in that the number of plies of described small pieces graphene film (2) is 1 layer to 20 layers.
The preparation method of 11. graphene films according to claim 1, is characterized in that the number of plies of described small pieces graphene film (2) is 1 layer to 5 layers.
The preparation method of 12. graphene films according to claim 1, is characterized in that described small pieces graphene film (2) area is 1nm
2to 1000cm
2.
The preparation method of 13. graphene films according to claim 1, is characterized in that described small pieces graphene film (2) area is 1nm
2to 100mm
2.
The preparation method of 14. graphene films according to claim 1, is characterized in that the number of plies of the graphene film (5) that becomes at Grown is 1 layer to 20 layers.
The preparation method of 15. graphene films according to claim 1, is characterized in that the number of plies of the graphene film (5) that becomes at Grown is 1 layer to 5 layers.
The preparation method of 16. graphene films according to claim 1, the temperature that it is characterized in that growing graphene film (5) is 50 ° of C to 1000 ° of C.
The preparation method of 17. graphene films according to claim 1, the temperature that it is characterized in that growing graphene film (5) is 50 ° of C to 600 ° of C.
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